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Continuous process for the production of combinatorial libraries of materials

a technology of combinatorial libraries and continuous process, applied in chemical/physical/physical-chemical stationary reactors, liquid-gas reaction processes, chemical/physical processes, etc., can solve the problems of affecting the efficiency of the production process, and affecting the effect of the production process

Inactive Publication Date: 2003-02-20
3M INNOVATIVE PROPERTIES CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

An important consideration in making these arrays is that batch reactors suffer from poor heat transfer characteristics, which may have a detrimental effect on the materials produced in batch arrays.
For example in "living" anionic polymerizations, gelation and increased polydispersity, due to termination reactions or other side reactions, are examples of detrimental effects that can occur as a result of poor heat transfer and mixing.

Method used

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  • Continuous process for the production of combinatorial libraries of materials
  • Continuous process for the production of combinatorial libraries of materials

Examples

Experimental program
Comparison scheme
Effect test

example 1

Poly(isoprene-4-vinyl pyridine) block copolymer--10 L STR

[0122] This example illustrates that the composition of constituent blocks in a block copolymer, made from anionically polymerizable monomers can be varied with time in the continuous process. This concept can be used to generate large material libraries.

[0123] An initiator slurry was prepared by mixing 1267 ml of 1.3 M sec-butyl lithium in cyclohexane with 4094 g of oxygen-free toluene and stirred at room temperature for about 30 minutes. Purified isoprene monomer (pressure fed at a rate of 85.8 g / min), purified THF (pressure fed at a rate of 23 g / min) and purified toluene solvent (diaphragm-pumped at a rate of 123.8 g / min) were fed into zone 1 of the STR. The initiator slurry was introduced by peristaltic pump at a rate of 12.5 ml / min into zone 1 of the STR. A color change from clear to yellow was observed in zone 1 when the initiator solution contacted the monomer, and an exotherm resulted. The reaction temperature was kept...

example 2

Poly(styrene-4-vinyl pyridine) block copolymer--2L Glass STR

[0126] This experiment exemplifies that this invention can be extended to different size STRs. An initiator slurry was prepared by mixing 585 ml of 1.3 M sec-butyl lithium solution in 6049 g of O.sub.2-free toluene and continuously stirring at room temperature for about 30 minutes. The stirring was done under nitrogen to prevent stratification and oxygen contamination. Purified styrene monomer (pressure fed at a rate of 31.7 g / min) and purified toluene solvent (diaphragm-pumped at a rate of 154.9 g / min) were passed into zone 1 of the STR. The initiator slurry was introduced by peristaltic pump at a rate of 19.6 ml / min into zone 1 of the STR. The solids loading of this reaction was 44 wt % in styrene monomer. A color change, from clear to red-orange, was observed in zone 1 when the initiator solution contacted the monomer, and an exotherm resulted. The mixture temperature in zone 1 was kept at about 43.degree. C. by adjustin...

example 3

Poly(styrene-4-vinyl pyridine) block copolymer--2L Glass STR

[0129] This experiment exemplifies that by not allowing the reactor to achieve steady state after a process change unexpected midpoints between anticipated or selected library members can be obtained.

[0130] An initiator slurry was prepared by mixing 585 ml of 1.3 M sec-butyl lithium solution in 6049 g of O.sub.2-free toluene and continuously stirring at room temperature for about 30 minutes. The stirring was done under nitrogen to prevent stratification and oxygen contamination. Purified styrene monomer (fed by a reciprocating piston-pump at a rate of 31.7 g / min) and purified toluene solvent (fed by a reciprocating piston-pump at a rate of 154.9 g / min) were passed into zone 1 of the STR. The initiator slurry was introduced by peristaltic pump at a rate of 19.6 ml / min into zone 1 of the STR. The solids loading of this reaction was 44 wt % in styrene monomer. A color change, from clear to red-orange, was observed in zone 1 wh...

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Abstract

A system is provided wherein a plug flow reactor is used to make combinatorial libraries of materials. Examples of plug flow reactors include stirred tube reactors, extruders, and static mixers.

Description

[0001] The present invention relates to a scaleable continuous process for the production of combinatorial libraries of materials in a plug-flow reactor.BACKGROUND INFORMATION[0002] The use of a combinatorial approach for materials synthesis is a relatively new area of research aimed at using rapid synthesis and screening methods to build libraries of polymeric, inorganic or solid state materials. For example, advances in reactor technology have empowered chemists and engineers to rapidly produce large libraries of discrete organic molecules in the pursuit of new drug discovery, which have led to the development of a growing branch of research called combinatorial chemistry. Robotic driven parallel synthesizers consisting of arrays of small batch type reactors have been designed for such efforts (e.g., Chemspeed, Endeavor, Neptune, FlexChem, Reacto-Stations). These reactors synthesize milligram to gram quantities of materials, which can rapidly be screened or analyzed by various tec...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01J19/00B01J19/18B01J19/20B01J19/24C07B61/00C08F2/01C08F297/02C08G85/00C40B40/14C40B50/08C40B60/14
CPCB01J19/0046Y10T436/25875B01J19/1818B01J19/1862B01J19/20B01J19/2415B01J19/242B01J2219/00033B01J2219/00036B01J2219/00063B01J2219/00094B01J2219/00306B01J2219/00351B01J2219/00353B01J2219/00355B01J2219/00418B01J2219/00481B01J2219/00495B01J2219/00585B01J2219/0059B01J2219/00599B01J2219/00698B01J2219/00707B01J2219/00722B01J2219/00756C08F297/02C40B40/14C40B50/08C40B60/14Y10T436/25Y10T436/2575B01J19/1812B01J19/00
Inventor NELSON, JAMES MICHAELDAVIDSON, ROBERT STEPHENCERNOHOUS, JEFFREY JACOBANNEN, MICHAEL JOHNMCNERNEY, JAMES ROBERTFERGUSON, ROBERT WADEMAISTROVICH, ANTHONY ROBERTHIGGINS, JAMES ALAN
Owner 3M INNOVATIVE PROPERTIES CO
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